Microporous crystalline zeolite material (zeolite ITQ-22), synthesis method thereof and use of same as a catalyst

a technology of zeolite and microcrystalline zeolite, which is applied in the direction of physical/chemical process catalysts, silica-polymorphs, silicon compounds, etc., can solve the problems of reducing the selectivity of zeolite for the desired process, entail a considerable increase in gas, and the use of fluoride ions in the synthesis is less desirable from the industrial point of view than the use of ohsup>, so as to achiev

Inactive Publication Date: 2005-08-18
CONSEJO SUPERIOR DE INVESTIGACIONES CIENTIFICAS (CSIC) +1
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Benefits of technology

[0013] The pore topology of this new zeolite confers on it properties for acting as an additive of zeolite faujasite Y in catalysts for fluid catalytic cracking (FCC) units, providing ...

Problems solved by technology

Nevertheless, the use of fluoride ions in the synthesis is less desirable from the industrial point of view than the use of OH−, given that the presence of fluoride ions requires the use of special materials in the synthesis equipment as well as specific treatment of the waste waters an...

Method used

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  • Microporous crystalline zeolite material (zeolite ITQ-22), synthesis method thereof and use of same as a catalyst
  • Microporous crystalline zeolite material (zeolite ITQ-22), synthesis method thereof and use of same as a catalyst

Examples

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example 1

[0090] This example illustrates the preparation of the dihydroxide of 1,5-bis(methylpyrrolidinium)pentane. In a 500 ml flask, 18.7 g of 1,5-dibromopentane, 20 g of 1-methylpyrrolidine and 300 ml of acetone are mixed. The mixture is left to reflux for 24 hours, after which the precipitated solid is separated by decantation and then washed several times with acetone. Finally it is vacuum dried and 31.9 g of a white solid are obtained. The analysis of elements and the nuclear magnetic resonance spectrum in D2O of this solid indicate that it is the desired product, namely, 1,5-bis(methylpyrrolidinium)pentane dibromide. The dihydroxide form of the structure directing agent is obtained by means of anion exchange using a Dowex SBR resin (in molar excess). The exchange is carried out with stirring of the fluid bed of resin in hydroxide form and an aqueous solution of the bromide of the cation for one night. The solution obtained is titrated with HCl (aq.) using phenolphthalein as indicator,...

example 2

[0091] This example illustrates the preparation of ITQ-22 by means of using the cation 1,5-bis(methylpyrrolidinium) pentane.

[0092] 6.17 g of tetraethylorthosilicate (TEOS) are added to 23.14 g of a solution of 1,5-bis(methylpyrrolidinium) pentane dihydroxide (R(OH)2) containing 0.96 equivalents of hydroxide in 1000 g. In this mixture 1.55 g of germanium oxide are added, and it is left to evaporate with stirring until complete elimination of the ethanol deriving from the hydrolysis of the TEOS plus the necessary quantity of water so that the final composition of the gel is: [0093] 0.67 SiO2: 0.33 GeO2: 0.25 R(OH)2:3.5 H2O

[0094] The mixture obtained is introduced into an autoclave internally lined with polytetrafluoroethylene and is heated at 175° C. for 14 days. The autoclave is then cooled, the contents are filtered, the solid is washed with water and dried at 100° C. The X-ray diffraction pattern is shown in FIG. 1 and the list of the most characteristic peaks appears in Table II...

example 3

[0095] The following example illustrates the preparation of ITQ-22 of different composition.

[0096] 12 g of tetraethylorthosilicate (TEOS) are added to 27.3 g of a solution of 1,5-bis(methylpyrrolidinium) pentane dihydroxide (R(OH)2) containing 1.16 equivalents of hydroxide in 1000 g. In this mixture 0.6 g of germanium oxide are dissolved, and it is left to evaporate with stirring until complete elimination of the ethanol formed plus the excess of water so that the final composition is as follows: [0097] 0.91 SiO2:0.09 GeO2:0.25 R(OH)2:3.5 H2O

[0098] The mixture obtained is heated in autoclaves internally lined with polytetrafluoroethylene at 175° C. for 14 days. The solid obtained after filtering, washing with distilled water and drying at 100° C. is ITQ-22.

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Abstract

The present invention refers to a microporous crystalline material of zeolitic nature (ITQ-22) which, in the calcined state, has the empirical formula wherein M is H+ or at least one inorganic cation of charge +n; X is at least one chemical element of oxidation state +3, preferably selected from the group consisting of Al, Ga, B, Fe and Cr; Y is at least one chemical element with oxidation state +4 other than Si and Ge, preferably selected from the group consisting of Ti, Sn and V; x has a value less than 0.2, preferably less than 0.1 and can take the value zero, y has a value less than 0.1, preferably less than 0.05 and can take the value zero, z has a value less than 0.8, preferably between 0.005 and 0.5 and can take the value zero, with a characteristic X-ray diffraction pattern, to the method of preparation and to the use of the material in separation and transformation processes of organic compounds.

Description

RELATED APPLICATIONS [0001] The present application is a Continuation of co-pending PCT Application No. PCT / ES03 / 00246, filed May 23, 2003, which in turn, claims priority from Spanish Application Serial Nos. P200201249, filed May 23, 2002, No. P200300444, filed Feb. 14, 2003, and No. P200301058, filed Apr. 30, 2003. Applicants claim the benefits of 35 U.S.C. §120 as to the PCT application and priority under 35 U.S.C. §119 as to said Spanish applications, and the entire disclosures of the applications are incorporated herein by reference in their entireties.TECHNICAL FIELD OF THE INVENTION [0002] This invention belongs to the technical field of microporous crystalline materials of zeolitic nature, useful as catalysts or components of catalysts for separation and transformation processes of organic compounds. STATE OF THE ART PRIOR TO THE INVENTION [0003] Zeolites are microporous crystalline materials formed from a crystal lattice of TO4 tetrahedra which share all their vertices givin...

Claims

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Application Information

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IPC IPC(8): B01J29/04B01J29/89C01B37/02C01B39/06C01B39/08C10G29/20C10G45/64C10G50/00
CPCB01J29/04B01J29/89C01B37/02C10G50/00C01B39/08C10G29/205C10G45/64C01B39/06
Inventor CANOS, AVELINO CORMAGARCIA, FERNANDO REYVALENCIA, SUSANA VALENCIAMARTINEZ TRIGUERO, LUIS JOAQUIN
Owner CONSEJO SUPERIOR DE INVESTIGACIONES CIENTIFICAS (CSIC)
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